CN111517331A - Method for preparing glass fiber raw material by modifying steel slag - Google Patents
Method for preparing glass fiber raw material by modifying steel slag Download PDFInfo
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- CN111517331A CN111517331A CN202010374788.8A CN202010374788A CN111517331A CN 111517331 A CN111517331 A CN 111517331A CN 202010374788 A CN202010374788 A CN 202010374788A CN 111517331 A CN111517331 A CN 111517331A
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- steel slag
- carbon black
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/162—Ammonium fluoride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/22—Fluorides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Geology (AREA)
- Processing Of Solid Wastes (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a method for preparing a glass fiber raw material by modifying steel slag, which comprises the following steps: (1) transferring the reactant of the ammonia water and the fluosilicic acid into a filter press, collecting filtrate, wherein the filtrate contains ammonium fluoride, and performing counter-current washing to obtain a byproduct white carbon black; feeding the washed white carbon black into a flash evaporation machine to obtain finished white carbon black; (2) adding ammonium fluoride into the crushed steel slag, filtering the filtrate after reaction to obtain steel slag modified filtrate, and recovering ammonia gas; washing the modified steel slag in a counter-current manner; (3) heating the filtrate to boil and volatilize ammonia gas, absorbing ammonia gas with water to obtain ammoniaThe water is recycled; washing the obtained white carbon black in a counter-current manner, and then performing flash evaporation to obtain a finished product of the white carbon black; and (4) returning the residual filtrate to the step (1) for recycling. The method for preparing the glass fiber raw material by modifying the steel slag provides a new way for recycling the steel slag, and the original calcium silicate form in the steel slag is modified into CaF by utilizing the existing fluosilicic acid and the solid waste steel slag2And SiO2And is used for preparing glass fiber raw materials.
Description
Technical Field
The invention belongs to the technical field of steel slag recovery, and particularly relates to a method for preparing a glass fiber raw material by modifying steel slag.
Background
The steel slag is derived from gangue and compounds generated by additives in ores or refined ores in the steel-making process, is industrial solid waste, is usually discarded as waste, occupies land and pollutes the environment; the steel slag contains useful components such as silicon, iron, aluminum and the like, so that the comprehensive development and utilization of the steel slag are well realized, resources and energy sources can be saved, and the occupied area of slag discharge and the pollution to the environment can be reduced; the steel slag is mainly used as metallurgical raw material (sintering flux, blast furnace or cupola furnace flux), building material (producing cement, broken stone and fine aggregate) and other uses (sewage treatment in environment and agriculture). The method for searching the new method for treating the steel slag improves the efficiency, realizes the effective utilization of resources and has obvious practical significance.
Disclosure of Invention
The invention provides a method for preparing a glass fiber raw material by modifying steel slag, which utilizes the existing fluosilicic acid and solid waste steel slag to modify the original calcium silicate form in the steel slag into CaF2And SiO2(ortho silicic acid) to achieve the purpose of meeting the glass raw material. The specific technical scheme is as follows:
the method for preparing the glass fiber raw material by modifying the steel slag comprises the following steps of:
(1) ammonium fluoride byproduct white carbon black prepared by fluorosilicic acid
Adding ammonia water with the mass concentration of 10-28% and the mass concentration of 20m into a reaction kettle3-25m3Slowly adding fluosilicic acid with the mass concentration of 20-40 percent into the mixture under the condition of continuous stirring3-12.5m3Controlling the pH value of the end-point solution to be 7-8 by ammonia water after the addition is controlled to be finished for 30-60 min;
transferring the reactant into a filter press, collecting filtrate containing ammonium fluoride, washing the byproduct white carbon black six times in counter current, wherein the water used for washing each time is not more than 1.2m3-2.3m3The washing liquid and the filtrate in the first two times are combined for use, and the washing is continued for the next four times; filtering the washed white carbon black, and feeding the filtered white carbon black into a flash evaporation machine through a spiral feeder to obtain a finished product white carbon black;
(2) modification of steel slag
Adding ammonium fluoride solution with the mass concentration of 30-40% for 10m into a reaction kettle3-16m3Adding 10t of steel slag crushed to 120 meshes under continuous stirring, continuously stirring and reacting for 3h, filtering the filtrate to obtain steel slag modified filtrate, and reserving recovered ammonia gas to prepare white carbon black; countercurrent washing machine
Washing the filtrate for six times, and performing step (3) to recover ammonia gas to prepare white carbon black;
(3) recycling of ammonium fluoride from washing filtrate and preparation of white carbon black
In a reaction kettle, modifying the steel slag obtained by filtering to obtain 10m of modified filtrate3Slowly adding 10-28% ammonia water 4m under continuous stirring3-10m3And after 30-60 min, 1.0t of precipitated white carbon black and a recovered ammonium fluoride solution containing 33% can be obtained for directly using the steel slag modification in the second step of circulation. Washing the obtained white carbon black in a counter-current manner, filtering the washed white carbon black, and then feeding the white carbon black into a flash evaporation machine through a spiral feeder to obtain a finished product of the white carbon black; and (4) returning the residual filtrate to the link of preparing ammonium fluoride by using the fluorosilicic acid and by-producing the white carbon black in the step (1) for recycling.
In the process of the method, siliceous materials in the materials are converted into valuable white carbon black, the silicon content in the steel slag is correspondingly reduced, and subsequent silicon supplement is required. If the preparation of the white carbon black is not needed, the steel slag modification in the step (2) and the recovery of ammonium fluoride from the filtrate in the step (3) can be combined with the preparation of the white carbon black, and the steel slag modification and the recovery of the ammonium fluoride can be simultaneously carried out, namely, the steel slag modification is carried out by slowly adding the steel slag into ammonia water under continuous stirring, at the moment, siliceous materials in the materials enter the steel slag in a form of the white carbon black for silicon supplement, and the white carbon black cannot be.
The method for preparing the glass fiber raw material by modifying the steel slag provides a new way for recycling the steel slag, and the original calcium silicate form in the steel slag is modified into CaF by utilizing the existing fluosilicic acid and the solid waste steel slag2And SiO2And is used for preparing glass fiber raw materials.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a schematic diagram of a counter current washing process.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiment.
Example 1
As shown in figure 1, the method for preparing the glass fiber raw material by modifying the steel slag comprises the following steps:
(1) ammonium fluoride byproduct white carbon black prepared by fluorosilicic acid
Adding 28% ammonia water 15m into the reaction kettle3Slowly adding 9.5m of 40 percent fluosilicic acid under continuous stirring3After the addition of 40min is finished, the pH value of the solution is controlled to be 7-8 (if the pH value is less than 7, the solution is neutralized to 7-8 by ammonia water).
The reaction mass is transferred to a filter press and the filtrate is collected, this liquid containing 33% of ammonium fluoride 25m3And the product is used for next modification of steel slag. The white carbon black as a byproduct is washed by countercurrent for six times, and the water consumption for each washing is 2.0m3The first two washes were combined with the filtrate and the next four washes were continued. And (3) filtering the washed white carbon black, and enabling the solid phase to enter a flash evaporation machine through a spiral feeder to obtain a finished product of white carbon black of 2.3 t.
In the counter-current washing process, as shown in fig. 2, the original leached waste is contacted with the leachate, the waste depleted in leaching is contacted with the fresh leaching agent, and the direction of the leaching agent is opposite to that of the leached waste, so that the residual leaching agent in the leachate can be fully utilized, the content of the target component in the leachate is high, the consumption of the leaching agent is low, but the leaching speed is low, the leaching time is long, more leaching stages are needed, the efficiency is high, and the operation is troublesome.
The countercurrent washing process is realized in a filter press, the water consumption of each time is 0.5-1 time of the solid content), such as 9.5m of 30 percent fluosilicic acid3With 25% ammonia water 25m3Reacting to obtain impure hydrated white carbon black with water content of 3t-6t and water consumption of 2.0m for each washing3And the washing liquid and the filtrate are combined for use in the first two times, and the washing liquid and the filtrate are continuously used for washing the white carbon black of the next batch for the last four times. And feeding the washed white carbon black into a flash evaporation machine through a spiral feeder to obtain a finished product of the white carbon black of 2.3 t. The remaining filtrate of the first two washing solutions was 4m3And returning to the link of preparing ammonium fluoride and preparing the byproduct white carbon black from the fluosilicic acid for recycling.
Ideally, after the first filter pressing of 3t-6t of white carbon black containing 55% of ammonium fluoride, the water content is 50%, the ammonium fluoride is contained by 0.58t, after the first washing, the ammonium fluoride is contained by 0.29t, after the six washing, the ammonium fluoride is contained by 0.009t, namely the ammonium fluoride content in the white carbon black after the six washing is 0.4%.
(2) Modification of steel slag
Adding 33% ammonium fluoride solution 25m into the reaction kettle3Adding 10t of steel slag crushed to 120 meshes under continuous stirring, reacting for 3 hours under continuous stirring, and filtering the filtrate to obtain 8.3m of steel slag modified filtrate3And the recovered ammonia gas is reserved for preparing the white carbon black. And (4) washing for six times in a counter-current manner, and leaving the washing filtrate for the next step of recycling ammonia gas to prepare the white carbon black.
The modified steel slag is also washed for six times, contains partial volatile ammonium fluoride and has the problem of volatilization in the subsequent high-temperature smelting process. If the washing is carried out for ten times, the ammonium fluoride in the material can be reduced to 0.00056 t.
(3) Recycling of ammonium fluoride from washing filtrate and preparation of white carbon black
In a reaction kettle, the steel slag modified filtrate obtained by filtering is 8.3m3Slowly adding 20% ammonia water 6m under continuous stirring3After 50min, 1.0t of precipitated silica and a solution containing 33% of recovered ammonium fluoride can be obtained for directly using the steel slag modification in the second step of circulation. And filtering the precipitated white carbon black and then carrying out flash evaporation to obtain a finished product of the white carbon black.
In the process of the method, siliceous materials in the materials are converted into valuable white carbon black, the silicon content in the steel slag is correspondingly reduced, and subsequent silicon supplement is required. If the preparation of the white carbon black is not needed, the steel slag modification in the step (2) and the recovery of ammonium fluoride from the filtrate in the step (3) can be combined with the preparation of the white carbon black, and the steel slag modification and the recovery of the ammonium fluoride can be simultaneously carried out, namely, the steel slag modification is carried out by slowly adding the steel slag into ammonia water under continuous stirring, at the moment, siliceous materials in the materials enter the steel slag in a form of the white carbon black for silicon supplement, and the white carbon black cannot be.
Example 2
As shown in figure 1, the method for preparing the glass fiber raw material by modifying the steel slag comprises the following steps:
(1) ammonium fluoride byproduct white carbon black prepared by fluorosilicic acid
Adding 25% ammonia water into the reaction kettle for 18t, and slowly adding 30% fluosilicic acid for 12.5m under continuous stirring3After the addition of 40min is finished, the pH value of the solution is controlled to be 7-8 (if the pH value is less than 7, the solution is neutralized to 7-8 by ammonia water).
The reaction mass is transferred to a filter press and the filtrate is collected, this liquid containing 30% of ammonium fluoride 28m3And the product is used for next modification of steel slag. The white carbon black as a byproduct is washed by countercurrent for six times, and the water consumption for each washing is 2.0m3The first two washes were combined with the filtrate and the next four washes were continued. And feeding the washed white carbon black filter residue into a flash evaporation machine through a spiral feeder to obtain a finished product of white carbon black of 2.3 t.
In the counter current washing process shown in figure 2, the raw leached waste is contacted with the leach solution, while the leach-depleted waste is contacted with fresh lixiviant, which is in the opposite direction to the direction of movement of the leached waste.
The countercurrent washing process is realized in a filter press, and the water consumption for each washing is 2.0m3And the washing liquid and the filtrate are combined for use in the first two times, and the washing liquid and the filtrate are continuously used for washing the white carbon black of the next batch for the last four times. And feeding the washed white carbon black into a flash evaporation machine through a spiral feeder to obtain a finished product of the white carbon black of 2.3 t. The remaining filtrate of the first two washing solutions was 4m3And returning to the link of preparing ammonium fluoride and preparing the byproduct white carbon black from the fluosilicic acid for recycling. Ideally, the ammonium fluoride in the white carbon black is 0.009t after six times of washing.
(2) Modification of steel slag
Adding 30% ammonium fluoride solution 28m into a reaction kettle3Adding 10t of steel slag crushed to 120 meshes under continuous stirring, reacting for 3 hours under continuous stirring, and filtering the filtrate to obtain 10m of steel slag modified filtrate3. And washing for six times in a counter current manner, and reserving washing filtrate for the next step of recovering ammonium fluoride and preparing white carbon black.
The modified steel slag is also washed for six times, contains partial volatile ammonium fluoride and has the problem of volatilization in the subsequent high-temperature smelting process. If the washing is carried out for ten times, the ammonium fluoride in the material can be reduced to 0.00056 t.
(3) Recycling of ammonium fluoride from washing filtrate and preparation of white carbon black
In a reaction kettle, modifying the steel slag obtained by filtering to obtain 10m of modified filtrate3Slowly adding 28% ammonia water 4.5m under continuous stirring3After 30min, 1.0t of precipitated silica and a solution containing 33% of recovered ammonium fluoride can be obtained for directly using the steel slag modification in the second step of circulation. Washing and filtering the precipitated white carbon black, and then performing flash evaporation to obtain a finished product of the white carbon black.
In the process of the method, siliceous materials in the materials are converted into valuable white carbon black, the silicon content in the steel slag is correspondingly reduced, and subsequent silicon supplement is required. If the preparation of the white carbon black is not needed, the steel slag modification in the step (2) and the recovery of ammonium fluoride from the filtrate in the step (3) can be combined with the preparation of the white carbon black, and the steel slag modification and the recovery of the ammonium fluoride can be simultaneously carried out, namely, the steel slag modification is carried out by slowly adding the steel slag into ammonia water under continuous stirring, at the moment, siliceous materials in the materials enter the steel slag in a form of the white carbon black for silicon supplement, and the white carbon black cannot be.
Claims (4)
1. The method for preparing the glass fiber raw material by modifying the steel slag is characterized in that the ammonium fluoride byproduct white carbon black is prepared by using fluosilicic acid and ammonia water, and each raw material comprises the following steps according to the following mixture ratio:
adding ammonia water with the mass concentration of 10-28% to a reaction kettle for 15m3Slowly adding fluosilicic acid with the mass concentration of 20-40 percent into the mixture under the condition of continuous stirring3Controlling the pH value of the end-point solution to be 7-8 by ammonia water after the addition is controlled to be finished for 30-60 min;
transferring the reactant into a filter press, collecting filtrate, wherein the filtrate contains ammonium fluoride, washing the byproduct white carbon black in a counter-current manner, and feeding the washed white carbon black into a flash evaporation machine through a screw feeder to obtain the finished product white carbon black.
2. The method for preparing the glass fiber raw material by modifying the steel slag according to claim 1, further comprising the following steps: adding ammonium fluoride solution with the mass concentration of 30-40% for 10m into a reaction kettle3-16m3Adding 10t of steel slag crushed to 120 meshes under continuous stirring, continuously stirring and reacting for 3h, filtering the filtrate to obtain steel slag modified filtrate, and reserving and recycling ammonia gas or preparing white carbon black; and washing the modified steel slag in a counter-current manner.
3. The method for preparing the glass fiber raw material by modifying the steel slag according to claim 2, further comprising the following steps:
in a reaction kettle, slowly adding 20 percent ammonia water 6m into the steel slag modified filtrate obtained by filtering under the condition of continuous stirring3After 50min, 1.0t of precipitated silica and a solution containing 33% of recovered ammonium fluoride of 10m can be obtained3The modified slag is directly used for modifying the circulating steel slag;
in the modification process of the steel slag, siliceous materials in materials are converted into valuable white carbon black, the obtained white carbon black is washed in a counter-current mode, filtered, washed and filtered white carbon black, and enters a flash evaporation machine through a spiral feeder to obtain a white carbon black finished product; the residual filtrate is recycled;
the silicon content in the steel slag is correspondingly reduced, and subsequent silicon supplement is needed; if the white carbon black does not need to be prepared, the steel slag modification and the ammonium fluoride recovery from the filtrate can be combined with the white carbon black preparation, the steel slag modification and the ammonium fluoride recovery can be simultaneously carried out, namely, the steel slag modification is carried out by slowly adding the steel slag into ammonia water under continuous stirring, at the moment, siliceous materials in the materials enter the steel slag in the form of the white carbon black for silicon supplement, and the white carbon black preparation cannot be recovered.
4. The method for preparing the glass fiber raw material by modifying the steel slag according to claim 3, wherein the byproduct white carbon black is washed by countercurrent for six times, and the water used for washing each time is not more than 2.5m3The washing liquid and the filtrate in the first two times are combined for use, and the washing is continued for the next four times; the modified steel slag is washed for six times in a counter current manner.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115709998A (en) * | 2022-11-14 | 2023-02-24 | 国能龙源环保有限公司 | Method for preparing white carbon black by roasting waste wind power blades |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115709998A (en) * | 2022-11-14 | 2023-02-24 | 国能龙源环保有限公司 | Method for preparing white carbon black by roasting waste wind power blades |
| CN115709998B (en) * | 2022-11-14 | 2023-03-31 | 国能龙源环保有限公司 | Method for preparing white carbon black by roasting waste wind power blades |
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Application publication date: 20200811 |